Process for the production of a liquid coffee concentrate

ABSTRACT

The present disclosure relates to a process for the production of a liquid coffee concentrate that has an improved storage stability at ambient temperature. The process comprises separating coffee extract resulting in a high aromatic coffee extract and a low aromatic coffee extract and subjecting the low aromatic coffee extract to a heat treatment and, optionally, a pH rising step.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a divisional of U.S. patent application Ser. No.14/170,358, filed on Jan. 31, 2014, which is a continuation ofInternational Patent Application No. PCT/NL2012/050543, filed on Aug. 1,2012, which claims the benefit of priority to European PatentApplication No. 11176077.3, filed on Aug. 1, 2011, the contents of whichare incorporated herein by reference in their entireties.

FIELD

The invention relates to a process for the production of a liquid coffeeconcentrate that has an improved storage stability at ambienttemperature.

BACKGROUND

Liquid coffee, and liquid coffee concentrates, are increasingly indemand for commercial and/or industrial purposes. The production andsales of liquid coffee, e.g. liquid coffee concentrates for use incoffee dispensing machines, makes it desirable to provide liquid coffeethat has a sufficient shelf-life. Up to now, such liquid coffee productsare mostly available in a frozen form, and sometimes refrigerated.Non-refrigerated storage would decrease supply chain costs. However, anyproducts sold for non-refrigerated storage still have an undesirablyshort shelf-life.

Generally speaking, a liquid coffee (such as a concentrate or anextract) is unstable over time and becomes increasingly acidic at roomtemperature. As is known by the skilled person, the pH drop might be dueto microbial action and to chemical reaction, such as a slow hydrolysisreaction of some compounds such as esters and lactones, oxidation ofcarbonyl group containing compounds or even the Maillard reactionoccurring among polysaccharides and proteins. A pH of 4.8 is commonlyconsidered in literature as the lower limit for taste acceptability.Below that pH level the coffee extract becomes undrinkable.

To overcome microbial acidification the liquid coffee is often treatedby UHT (Ultra High Temperature). Particularly suitable UHT treatment isat 120° C. for a couple of seconds.

A reference addressing the chemical acidification is US 2010/0316784.Therein a treatment is proposed comprising adding an edible alkalisource to a liquid coffee concentrate. This serves to artificiallyincrease pH. Before or after the addition of alkali, a heat treatment isconducted so as to artificially drive acid-generation reactions in thecoffee concentrate to completion. More particularly, the heat treatmentis conducted between 140 and 146° C. at a holding time of at most 3minutes. This method fails, however, to produce products of sufficientshelf-life and quality.

Another drawback of the aforementioned process is the addition ofalkali. In many jurisdictions, such an addition is considered undesiredand/or the resulting product is no longer entitled to be called a“coffee,” like under the EC food regulations. It would be desirable todevelop a process for making liquid coffee whereby the addition ofingredients other than those obtained from a coffee extract itself isunnecessary, and yet provide a storage stable liquid coffee concentrateof good flavor qualities.

Another reference addressing the stabilization of liquid coffee bytreatment with alkali is EP 861 596. Herein a coffee extract is treatedwith an alkali, which is present in an amount effective to convert acidprecursors present in the coffee extract to their respective acid salts,and thereafter neutralizing the treated coffee extract with an acid, inan amount sufficient to neutralize any excess alkali from the firststep. Apart from the aforementioned drawback of using alkali, thismethod also adds acid, which increases the amount of foreign componentspresent in the liquid coffee. Moreover, the method is essentially basedon introducing ionic substances (salts) which are prone to adverselyaffect taste.

Yet another reference addressing shelf life of liquid coffees is EP 1374 690. Herein a coffee extract is subjected, essentially immediatelyafter preparation, to correction of acidity by the addition of a base oran anion resin. The resulting extract is subjected to pasteurisation.The pasteurisation is discussed with reference to holding times andtemperatures that do not affect the organoleptic properties of thecoffee extract. A typical temperature range is 100° C.-140° C. at aholding time of at most 1 minute. This method fails also to produceproducts of sufficient shelf-life and quality.

The object of the present invention is to provide a process with whichan improvement of the quality of the coffee concentrate is obtained instorage stability as well as in flavor.

SUMMARY

In order to better address one or more of the foregoing desires, thedisclosure, in one aspect, presents a process for the production of aliquid coffee concentrate with a pH of 4.8 to 6 comprising the steps of:

-   -   a) subjecting roasted, ground coffee to one or more extraction        steps with water resulting in a coffee extract,    -   b) separating the coffee extract, either by fractionation during        the extraction step(s) in a) or by aroma recovery after step a)        resulting in a high aromatic coffee extract and a low aromatic        coffee extract,    -   c) subjecting at least 50% of the low aromatic coffee extract to        a heat treatment of at least 120° C. at a holding time for at        most 30 minutes,    -   d) concentrating at least the treated low aromatic coffee        extract,    -   e) combining at least the concentrated low aromatic coffee        extract with the high aromatic coffee extract,    -   thereby obtaining a liquid coffee concentrate.

In another aspect, the disclosure provides a liquid coffee concentratewith a pH of 4.8 to 6 obtainable by the above-mentioned process.

BRIEF DESCRIPTION OF THE FIGURES

FIG. 1 is a chart depicting the pH level versus time for a liquid coffeeconcentrate prepared in accordance with Example 2 herein, according toone embodiment.

FIG. 2 is a chart depicting characteristics of the liquid coffeeconcentrate of Example 2 in response to various temperature and timetreatments, according to one embodiment.

FIG. 3 is a chart depicting the pH level versus time for a liquid coffeeconcentrate prepared in accordance with Example 4 herein, according toone embodiment.

FIG. 4 is a chart depicting the pH level versus time for a liquid coffeeconcentrate prepared in accordance with Example 6 herein, according toone embodiment.

FIG. 5 is a flow chart of a process of making a coffee concentrate,according to one embodiment.

FIG. 6 is a flow chart of a process of making a coffee concentrate,according to another embodiment.

DETAILED DESCRIPTION

In a broad sense, the invention is based on the judicious insight toconduct a relatively strong heat treatment at a certain holding time ona coffee extract wherefrom aroma components have been recovered prior toconcentration. Further, the invention provides, preferably, a judiciouscombination of such a heat treatment step and a pH-rising treatment.More preferably, the pH rising step does not involve the addition ofalkali. Most preferably, the process results in a hydrolysation of atleast 150 mmoles acid/kg dry matter solids content in the final product.This is the difference between the amount of mmoles/kg dry matter solidscontent in the low aromatic coffee extract to be treated before andafter the heat treatment multiplied by the wt/wt ratio dry matter solidscontent of the low aromatic coffee extract in the final product.

The coffee chosen for the extraction in step a) can be any type ofroasted coffee. The provision of roasted coffee is well-known to theskilled person. For example, the starting material can be a customarycoffee bean raw material for industrial extraction processes, whichcoffee origins are roasted in the customary manner. As a rule, to thatend, a mixture of different types of coffee origins is used. The roastedcoffee beans are ground, while generally, for the degree of grinding acompromise is sought between obtaining the largest possible surface andobtaining a lowest possible pressure drop across the extraction cell. Asa rule, the ground beans have an average size of 2.0 millimeters.

In order to better preserve coffee aromas, the process of the presentinvention is conducted on a low aromatic coffee extract. This isobtained by a) subjecting roasted, ground coffee to one or moreextraction steps with water resulting in a coffee extract, and b)separating the coffee extract, either by fractionation during theextraction step(s) in a) or by aroma recovery after step a) resulting ina high aromatic coffee extract and a low aromatic coffee extract.

Examples of aroma recovery after step a) include steam stripping,supercritical CO₂ extraction, and pervaporation. In another embodiment,the coffee extract is fractionated during the extraction step a). Thespecific coffee aroma, present in the high aromatic coffee extractresulting therefrom, has a more natural coffee character compared tocoffee aroma recovered by means of steam stripping from the completeextract after step a). A high aromatic coffee extract and a low aromaticcoffee extract are obtained. As known to a skilled man, a high aromaticcoffee extract distinguishes itself from a low aromatic coffee extractby having a comparably high amount of volatile flavor compounds comparedto semi volatile flavor compounds. Such compounds are known for examplefrom Clarke R. J. and Vitzthum O. G., Coffee Recent Developments, 2001(ISBN 0-632-05553-7), p. 71, table 3.3. From this table it is clear thaton the one hand propanal, methyl propanal, and 2,3 butanedione aremeasurable volatile flavor compounds. Pyrazine compounds and guaiacolcompounds on the other hand are semi volatile flavor compounds. Takinge.g. 2,3-butanedione as an example of a volatile coffee flavor compoundand ethyl guaiacol (4-ethyl 2-methoxyphenol) as an example of a semivolatile coffee flavor compound, when these compounds are in a wt/wtratio of 2,3-butanedione/ethyl guaiacol >30 in a particular coffeeextract, that extract can be described as a high aromatic coffeeextract. Consequently, a low aromatic coffee extract has a wt/wt ratioof 2,3-butanedione/ethyl guaiacol <30.

The high aromatic coffee extract is stored.

The low aromatic coffee extract is an undiluted or unconcentratedextract. Whilst, preferably, the treatment is conducted on an extract asis, it will be understood that a small change of the extract, byinsubstantial dilution or insubstantial concentration, will not deviatefrom the gist of the invention. This is markedly different from themethod disclosed in US 2010/0316784, where it is expressly required thatthe extract is concentrated prior to the heat treatment. An extract willgenerally have a dry matter solids content of 15% by weight or less,preferably of from 2 to 10% by weight. A concentrate is distinguishedfrom an extract by having undergone a substantial water removing stepsuch as water evaporation. Whilst a concentrate will generally have adry matter solids content of 6 wt. % to 80 wt. %, it will usually be atleast 10 wt. % higher in dry matter solids than the preceding extract,and regularly has a dry matter solids content of above 10 wt. %,particularly above 15 wt. %.

At least 50 v/v %, more preferably 75 v/v %, most preferably all (100%)of the low aromatic coffee extract is subjected to a heat treatment ofat least 120° C. at a holding time for at most 30 minutes, preferably ata temperature of at least 135° C. at a holding time of at most 15minutes, more preferably at least 150° C. at a holding time of at most10 minutes. In general, the higher the temperature the shorter theholding time. In particular, below 150° C. the holding time has to be atleast 10 minutes. In this respect, the above-mentioned publicationsteach away from the present invention as the temperatures and holdingtimes disclosed are below 150° C. and shorter than 3 minutes.Preferably, the heat treatment is conducted from 120° C. to 200° C. at aholding time of 30 minutes to 10 seconds. More preferably, the heattreatment is conducted from 135° C. to 180° C. at a holding time of 15minutes to 1 minute. Most preferably, the heat treatment is conductedfrom 150° C. to 180° C. at a holding time of 10 minutes to 1 minute. Asa particular example the heat treatment can be conducted at about 150°C. with a holding time of about 5 minutes.

Heating times may include heating from ambient temperature to theholding temperature during 1-8 minutes, preferably 3-5 minutes.

Cooling times may include cooling to ambient temperature during 1-8minutes, preferably 3-5 minutes.

In a preferred embodiment, the process comprises a pH rising step(de-acidification or pH adjustment step) after step b). This pH risingstep may be conducted before or after the concentration step d).Preferably, the pH rising step is conducted before the concentrationstep whereby the low aromatic extract is subjected to a pH rising step,i.e. the low aromatic extract is subjected to the pH rising step beforeor after the heat treatment step c).

With the pH-rising step the pH is raised to a less acidic (morealkaline) pH, preferably having a value of from 5-10.

This raise is relative to the starting pH. In other words, if thestarting pH is 4, the pH rise could be to a value that is still acidic,e.g. 5. However, preferably the starting pH of the coffee stream is 4.5to 6.5, more preferably of from 4.9 to 5.7. After the treatment stepsthe pH will again be at normal level such as between 4.8 and 6.

In a preferred embodiment of the process of the invention, the pH riseof the low aromatic extract is conducted prior to the heat treatment. Inthis embodiment it is further preferred that the pH is raised to a valueof 6 to 8. In another preferred embodiment, the pH rise is conductedafter the heat treatment. In this embodiment it is further preferredthat the pH is raised to a value of 5 to 7.

The pH-rising step can be conducted by adding edible alkali. Sources ofedible alkali are known, and have also been described in theaforementioned US 2010/0316784.

More preferably, however, the pH-rising step is conducted without addingalkali. By avoiding the addition of foreign substances, it is securedthat the product after treatment remains considered to be “coffee” inaccordance with the applicable food legislation in many jurisdictions.For, in such jurisdictions the addition of substances other than thoseobtained from the extraction will result in a product that is notallowed to be indicated as a coffee. It will be understood that such aproduct may receive a different perception by consumers. An underlyingtechnical problem thus is the provision of a process that sufficientlytreats the coffee so as to result in a product of sufficient storagestability and aroma quality, yet without the addition of foreignsubstances such as edible alkali.

This is secured in a preferred embodiment of the invention, wherein inthe pH rising step use is made of an ion exchange resin and/or anadsorber. The adsorber may be carbon based, polyacrylate based orpolystyrene based. Examples of commercial adsorbers include Purolite® MN200, Purolite® MN 202, and Lewatit® AF5. Examples of the ion exchangeresins include strong or weak basic anion exchange resins. Preferably,the ion exchange resin is a weak basic anion exchange resin. The resinis based on polyacrylate or polystyrene, preferably polyacrylate. Thefunctional groups are e.g. amine functional groups, such as primary,tertiary, and quaternary amine groups as well as polyamine groups,preferably tertiary amine groups. In the following table examples ofcommercial ion exchange resins are listed.

% of quaternary total gel/macro- functional amines capacity Name Matrixporous group (SBA) (eq/L) Rohm & Haas IRA 67 polyacrylic gel tertiaryamine 24% 1.6 Lewatit ® XA 945 Lewatit ® MP 62 polystyrene macroporoustertiary amine  3% 1.7 Purolite ® A 172 polystyrene gel tertiary amine 2% 1.2 Lewatit ® A 365 polyacrylic gel poly amine Lewatit ® VP OCpolyacrylic gel poly amine 14% 2.9 (3.4) 1075 Lewatit ® VP OCpolystyrene macroporous primary amine 2.2 1065 Lewatit ® MonoPluspolystyrene gel quaternary 100%  1.2 M 500 amine, Type I Lewatit ® M 600polystyrene gel quaternary 100%  1.1 amine, Type II

In the lower temperature ranges, viz. from 120° C. to below 150° C., thepH-rise is preferably effected prior to the heat treatment. Withoutwishing to be bound by theory, the present inventors believe that thepH-rise is capable of catalyzing acid-releasing reactions. The effectthereof is more pronounced in the lower regions of the heat treatmentconditions.

Preferably, the heat treatment is an extreme heat treatment in the sensethat it is conducted in the higher temperature ranges of 150° C. orabove. Here the process is more robust in the sense that the order aswell as the strength of the pH rising step is less critical. This hassignificant advantages not only creating a greater freedom of processing(viz. the order of the treatment steps), but also requiring a lesserdegree of de-acidification.

In connection with the addition of foreign substances such as ediblealkali, it is particularly preferred in this embodiment to choose theaforementioned conditions of extreme heat treatment. Thus, the additionof alkali can be minimized.

In the last steps the low aromatic coffee extract is concentrated.Preferred concentrates comprise 6 wt. % to 80 wt. % coffee solids,preferably 10 wt. % to 65 wt. %, more preferably 15 wt. % to 50 wt. %.Methods of concentration such as evaporating water are well-known to theskilled person.

In the event that part (i.e. at least 50%) of the low aromatic coffeeextract has been treated, the untreated low aromatic coffee extract maybe combined with the treated low aromatic coffee extract, i.e. beforeconcentration, or with the treated concentrated low aromatic coffeeextract, i.e. after concentration.

Generally, after concentration the concentrated treated low aromaticextract is mixed with the high aromatic extract. This can be done in thefactory before optionally further treatment steps and packaging or justbefore dosing by the consumer. In the latter case, two separate packagesare provided to the consumer to be introduced in the coffee preparingmachine.

In the factory, after temporary, preferably cooled, storage, preferablyat a temperature below 25° C., more preferably below 10° C., mostpreferably below 0° C., the high aromatic coffee extract may directly,without further processing, be added to the concentrated low aromaticcoffee extract. It is preferred that the high aromatic coffee extract isstored as briefly as possible and cooled, preferably at an atmosphere ofan inert gas such as nitrogen for adding to the concentrated lowaromatic coffee extract; owing to these steps loss of aroma and aromadegradation reactions are limited as much as possible.

Accordingly, the present process provides for a liquid coffeeconcentrate with a pH of 4.8 to 6 that can be stored at ambienttemperature (generally indicating a temperature of 5° C. to 25° C., andpreferably without the need for refrigerating equipment) at anacceptable shelf-life without acidification to occur, and capable ofbeing kept without substantial off-flavors to arise.

In a preferred embodiment, the extraction in step a) is preferably doneas a split extraction. Processes of split extraction are known. Areference in this respect is WO 2007/043873. More particularly, theprocess involves primary and secondary extraction.

In a preferred embodiment of split extraction, the invention is put touse in the following method for preparing a coffee concentrate. In themethod, roasted, ground coffee is subjected to a primary extraction withwater, whereby a first primary extract (i.e. the high aromatic coffeeextract) is obtained with a draw-off factor of at most 2.5, preferablyat most 2.0, more preferably at most 1.5 and most preferably at most1.0. Thereafter, optionally, a second primary extract is obtained.

The primarily extracted, roasted, ground coffee is then fed to asecondary extraction section in which, with water having a feedtemperature between 120 and 210° C., a secondary extract is obtained(the low aromatic coffee extract). At least 50 v/v %, more preferably 75v/v %, most preferably all (100%) of the secondary extract is thensubjected to the process steps of the present invention. Optionally, thesecond primary extract may be added to the secondary extract (the lowaromatic coffee extract) before or after the treatment step(s) of thepresent invention, preferably the second primary extract is added beforethe treatment to the secondary extract.

The term “draw-off factor” is understood to mean the ratio of the massof the extract and the mass of the dry roasted and ground coffee in theprimary extraction cell. In practice, this draw-off factor is determinedby a compromise between, on the one side, a sufficient degree of coffeearoma recovery in the first primary extract, and, on the other side, alowest possible volume of the first primary extract. The draw-off factorfor that matter depends on the used coarseness or degree of grinding ofthe roasted coffee, the extraction cell and, in particular, the numberof percolators placed in series, the used water-coffee ratio, the cycletime, the feed water temperature and the desired concentration of theend product and the like.

In a further preferred embodiment of split extraction, also a secondprimary extract is recovered from the primary extraction cell. To thatend, after draw-off and storage of the first primary extract, furtherextraction takes place in the primary extraction cell.

The recovery of both a first and second primary extract is particularlyattractive when a high water-coffee ratio is applied. Preferably, thewater-coffee ratio is between 5.0 and 15. More preferably, thewater-coffee ratio is lower than 10, and most preferably, thewater-coffee ratio is between 6.5 and 8.5.

When a second primary extract is recovered, preferably, the firstfraction of the secondary extract is indeed used as primary feed waterin the first extraction cell. For this embodiment, the teachings ofEP-A-0 352 842 are included herein by reference.

The second primary extract can be subjected to aroma recovery. Therecovered aromas are added to the high aromatic extract. The secondprimary extract after the aroma recovery may be added to the secondaryextract (the low aromatic coffee extract) before or after the treatmentstep(s) of the present invention, preferably the second primary extractis added before the treatment to the secondary extract. Afterconcentration the concentrated low aromatic coffee extract and the higharomatic coffee extract (comprising the recovered aromas) are combined.

In this embodiment of the invention, the primary extraction is carriedout with water at a feed water temperature which is lower than thatwhich is used in the secondary extraction. Preferably, the temperatureat which the primary extraction is carried out is between 70 and 120° C.

The primary extraction can be carried out as an exhaustive extraction.“Exhaustive extraction” is understood to mean that extraction takesplace until the extract hardly, if at all, differs from the waterintroduced into the extraction cell. In practice however, it will bebeneficial to the efficiency of the entire process, in particularbecause of the subsequent concentration steps, when extraction is notexhaustive.

“Water” for that matter is understood to include customary aqueoussolutions that can also be used in the known industrial extractionprocesses.

The primary and secondary extractions can be carried out in customaryextraction cells. In a preferred embodiment, both the primary and thesecondary extraction are carried out in a percolator or in percolatorsplaced in series. In particular, the secondary extraction isadvantageously carried out in at least 2, and preferably at least 4series-connected percolators. As a rule, the number of percolators usedin the primary extraction section is at least 0.5 which means thatduring 50% of the cycle time a percolator is connected in the primaryextraction section. Preferably, at least 1 or 2 percolators areconnected in the primary extraction section.

In a preferred embodiment of the process according to the invention, thelow aromatic coffee extract is at least part but preferably the total ofa secondary extract. In one further preferred embodiment hereof, thetreated low aromatic coffee extract is combined with a second primaryextract prior to the concentration step. In another preferred embodimenthereof, the low aromatic coffee extract is a mixture of at least partbut preferably the total secondary extract and the second primaryextract.

It has also been found that the second primary extract can be subjectedto the treatment of the present invention. In that respect, both thesecond primary extract and the secondary extract are considered the lowaromatic coffee extract of which at least part of the second primaryextract is treated which part to be treated comprises at least 25 v/v %,more preferably at least 35 v/v %, most preferably at least 50 v/v % ofthe low aromatic coffee extract. After the treatment, the treated partof the second primary extract is added to the non-treated part of thesecond primary extract and the secondary extract and concentrated.Preferably, all of the second primary extract is treated.

Preferred is also the use of customary liquid or dried fillercomponents. A filler component is sometimes used to neutralize themarked flavour character of the first primary extract to some extent.The filler is preferably a high yield coffee product. It may be added tothe low aromatic coffee extract before concentration, more preferablybefore the temperature treatment.

The invention also pertains to a liquid coffee concentrate with a pH of4.8 to 6 obtainable by the process of the invention. The liquid coffeeconcentrate comprises 6 wt. % to 80 wt. % coffee solids, preferably 10wt. % to 65 wt. %, more preferably 15 wt. % to 50 wt. %. This coffeeconcentrate is distinguished from coffee concentrates not according tothe invention, on account of its better storage stability at ambienttemperature, as can be identified with reference to the reduced, orpreferably absent, pH lowering, and to reduced, and preferably absentoccurrence of off-flavors. Preferably, the liquid coffee concentrate hasa storage stability of more than 6 months, more preferably more than 12months, most preferably more than 18 months.

A product treated by the process according to the present inventiondistinguishes itself by comprising at least 2 mg/kg dry matter of2-phenyl-3-(2-furyl)-2-propenal.

Accordingly, the present invention also relates to a liquid coffeeconcentrate with a pH of 4.8 to 6 comprising at least 2 mg/kg dry mattersolids of 2-phenyl-3-(2-furyl)-2-propenal, preferably between 4 mg/kgdry matter solids and 80 mg/kg dry matter solids, more preferablybetween 4 mg/kg dry matter solids and 40 mg/kg dry matter solids.

Alternatively, a product treated by the process according to the presentinvention distinguishes itself by having a QA/QaL mol/mol ratio between10 and 100 at a pH between 5 and 5.2. More particularly, during theshelf life the liquid coffee concentrate will enter a pH window between5 and 5.2. In that pH window it should have a QA/QaL mol/mol ratiobetween 10 and 100.

Accordingly, the present invention also relates to a liquid coffeeconcentrate with a pH between 5 and 5.2 and a QA/QaL mol/mol ratiobetween 10 and 100, preferably between 30 and 100, most preferably 60 to100. In a preferred embodiment, this liquid coffee concentrate will havea potassium content of 55 g or less per kg dry matter, preferably 20-55g/kg and/or a sodium content of 4 g or less per kg dry matter,preferably 0.1-4 g/kg.

The abbreviation QA stands for Quinic acid, i.e.1,3,4,5-tetrahydroxycyclohexanecarboxylic acid. The abbreviation QaLstands for Quinic acid lactone, i.e.1,3,4-trihydroxy-6-oxabicyclo[3.2.1]octan-7-one.

Various embodiments of the invention are further explained withreference to the Examples and Schemes 1 and 2, shown in FIGS. 5 and 6,which provide process schemes for implementing the treatment steps ofthe disclosure in processes for making coffee concentrates. Theseschemes serve illustrative purposes, and do not limit the invention.

In Scheme 1 (FIG. 5), a preferred embodiment of the invention isillustrated. Roasted coffee is subjected to split extraction, with splittapping (rendering first and second primary and secondary extractions).The second primary extract is combined with the second secondaryextract, and this stream is subjected, before concentration, to pHadjustment (by anion exchange), and extreme heat treatment (at theabove-identified temperatures). The concentrated extract is combinedwith the first primary extract resulting in a liquid coffee concentrateof the present invention.

Scheme 2 (FIG. 6) illustrates a further preferred embodiment. Therein,either the second secondary extract or the 2^(nd) primary extract orboth and mixtures thereof are subjected to the pH adjustment by anionexchange and heat treatment, before being combined with the firstprimary extract. The 2^(nd) primary extract may be subjected to aromarecovery, so that after concentration the concentrated coffee extract ismixed with 1^(st) primary extract as well as the aroma recovery product.Optionally, a filler component can be added either before or afterconcentration.

Analytical Method for QA and QaL

Quinic acid lactone (QaL), was obtained from Syncom, Groningen, theNetherlands. A working solution of approximately 0.5 mg per ml wasobtained by diluting QaL in acetonitrile. This working solution wasfurther diluted in 0.1% acetic acid in acetonitrile to obtaincalibration solutions of 15 ng/ml up to 15000 ng/ml.

Concentrated coffee products were diluted with water to 0.28% drymatter.

50 μl of the diluted coffee product is further diluted with 950 μl 0.1%acetic acid in acetonitrile.

Quantification was performed with a Triple Quad MS, TSQ Quantum Ultra;Thermo Scientific Mass spectrometer coupled to a Accela UPLC from ThermoScientific.

Concentrations were calculated from the calibration curve.

Quinic acid (QA), was obtained from Aldrich. A working solution ofapproximately 1 mg per ml was obtained by dissolving the compound inwater. This working solution was further diluted in 0.4 mMheptafluorobutyric acid to obtain calibration solutions of 10 μg/ml upto 40 μg/ml.

Concentrated coffee products were diluted with 0.4 mM heptafluorobutyricacid to 0.1% dry matter (w/w) dry coffee solids.

Quantification was performed with a Dionex ICS 5000 DC suppressedconductivity chromatograph.

Concentrations were calculated from the calibration curve.

Analytic method for 2-phenyl-3-(2-furyl)-2-propenal

2-phenyl-3-(2-furyl)-2-propenal, was obtained from Chemos GmbH,Werner-von-Siemens-Straβe, D-93128 Regenstauf, Germany (purity 97%). Aworking solution of 1 mg per ml was obtained by diluting the compound inhexane. This working solution was further diluted to obtain calibrationsolutions of 0, 0.6, 1, 3, 6, 10 and 50 μg2-phenyl-3-(2-furyl)-2-propenal per ml hexane.

Liquid coffee concentrates were diluted with water to 2.5% dry matter.

Volatiles in the coffee headspace were analysed by solid phasemicro-extraction (SPME) coupled to gas chromatography/mass spectrometry(GC/MS), essentially as described in Tikunov et al., 2005, PlantPhysiology 139, 1125-1137, was calculated from the linear calibrationcurve of the authentic standard in the coffee matrix.

Example 1 Extraction (Split Stream)

From a single batch of ground coffee, a coffee extract is obtained bysplit stream extraction as described in WO 2007/043873.

A 1^(st) primary extract (stream A in FIG. 5), which is high in flavor,the high aromatic coffee extract, is left untreated or concentrated andwill be added to the concentrated low aromatic coffee extract (stream H)prior to UHT treatment and packaging. All of the secondary extract ismixed with 2^(nd) primary extract (stream C). The resulting mixture(Stream G) is composed of 72.7% w/w secondary extract (stream E) and27.3% w/w 2^(nd) primary extract (stream C).

Adding Filler

An unconcentrated high yield extract (stream F) is made from a secondbatch of coffee. This high yield extract is directly added to the lowaromatic coffee extract. This results in a mixture of dry matter solidscontent of approximately 6%.

Processing

The pH of the low aromatic coffee extract is adjusted by passing theextract over an anion column (Lewatit® XA 945) to pH 8.

The low aromatic coffee extract is heated from ambient conditions to150° C. in 5 minutes, and kept at that temperature for 5 consecutiveminutes, followed by a cooling step of 3 minutes.

The heat treated low aromatic coffee extract is concentrated to a drymatter solids content of 28% by evaporation.

During these process steps >150 mMoles acid/kg dry matter solids contentis released by hydrolysis

The concentrated low aromatic coffee extract is mixed with the higharomatic coffee extract (1^(st) primary extract) (stream A).

Final Product

The resulting pH of the liquid coffee concentrate is 6.2

No detectable off flavor is detected in the liquid coffee concentrate.

During a shelf life of 8 weeks the liquid coffee concentrate is notperceived as acidified by a team of sensory experts.

By comparison, products manufactured according to the process describedin US 2010/0316784 do show acidification during this shelf life period.

Example 2

A single batch of Arabica coffee is subjected to the extraction asdescribed in Example 1. The primary extract, i.e. the high aromaticcoffee extract, comprises 16 wt. % of the total coffee dry matter andhas a BD/EG wt/wt ratio of 100. The low aromatic coffee extractcomprises 84 wt. % of the total coffee dry matter. The pH of the lowaromatic coffee extract obtained therefrom with a dry matter solidscontent of approximately 6% is adjusted by passing the extract over ananion column (Lewatit® XA 945) to pH 6. The amount of acids was assessedby titration up to pH 8. The low aromatic coffee extract having 287mmoles acid/kg dry matter is heated from ambient conditions to 160° C.in approximately 3.5 minutes, and kept at that temperature for 10consecutive minutes, followed by a cooling step of approximately 2minutes. The treated low aromatic coffee extract has 818 mmoles acid/kgdry matter. The heat treated low aromatic coffee extract isconcentrated. This process results in a hydrolysation of at least 446mmol acid/kg dry matter solids content in the final product((818−287)*0.84).

The concentrated low aromatic coffee extract is mixed with the higharomatic coffee extract (1^(st) primary extract) (stream A). Theresulting pH of the liquid coffee concentrate is 5.34. The liquidconcentrate has a dry matter solids content of 28%.

No detectable off flavor is detected in the liquid coffee concentrate.

The pH was followed in time as shown in FIG. 1 (▴). During 28 weeksshelf life the product does not drop in pH below 5. When assessed byexpert tasters, no unpleasant acidity can be detected in the product.

The liquid coffee concentrate comprises an amount of 7.5 mg/kg drymatter solids 2-phenyl-3-(2-furyl)-2-propenal.

The amount of potassium is 53 g/kg dry matter and the amount of sodiumis 2 g/kg dry matter. After 8 weeks storage the pH of the concentrate is5.1 and the QA/QaL mol/mol ratio is 90.

For comparison, a liquid coffee concentrate is prepared in the samemanner as described above except that the heat treatment is omitted. Theresulting liquid coffee concentrate has a pH of 5.2. Within 4 weeks,this product drops below pH 5 (see FIG. 1 (▪)). When assessed by experttasters the product is unpleasantly sour.

Example 3

Example 2 was repeated whereby the low aromatic coffee extract wassubjected to various temperature and time treatments. The experimentsare provided in FIG. 2. On the y axis is given the temperature indegrees Celsius at which coffee extracts were treated, the x axis givesthe duration of the heat-treatment in minutes. The numbers in FIG. 2indicate the amount of mMoles acid/kg dry matter solids content in thefinal product which is released by hydrolysis.

The “▪” marker of FIG. 2 indicates a coffee extract which yielded morethan 150 mMoles acid/kg dry matter solids content in the final productreleased by hydrolysis and thus are obtained with The process of theinvention

The “” marker of FIG. 2 indicates a coffee extract which yielded lessthan 150 mMole acid/kg dry matter solids content in the final productreleased by hydrolysis. Accordingly, these are comparative examples.

Example 4

A single batch of Arabica coffee is subjected to extraction wherebyaromas were fractionated from a highly aromatic coffee by means of steamdistillation as described in EP-A-0 352 842. This results in a steamdistillate, i.e. the high aromatic coffee extract (stream D) and a lowaromatic coffee extract comprising stream D′ and stream E in FIG. 6.

The pH of the low aromatic coffee extract with a dry matter solidscontent of approximately 5% is adjusted by passing the extract over ananion column (Lewatit® XA 945) to pH 6. The low aromatic coffee extractis heated from ambient conditions to 180° C. in 6 minutes, and kept atthat temperature for 1.5 consecutive minutes, followed by a cooling stepof 3 minutes.

The heat treated low aromatic coffee extract is concentrated. Thisprocess results in a hydrolysation of 395 mMoles acid/kg dry mattersolids content in the final product.

The concentrated low aromatic coffee extract is mixed with the higharomatic coffee extract (stream D).

The resulting pH of the liquid coffee concentrate is 5.35. The liquidconcentrate has a dry matter solids content of 28%.

No detectable off flavor is detected in the liquid coffee concentrate.

The pH was followed in time as shown in FIG. 3 (▴). During 7 weeks shelflife the product does not drop in pH below 5. When assessed by experttasters, no unpleasant acidity can be detected in the product.

The liquid coffee concentrate comprises an amount of 6 mg/kg dry mattercoffee solids 2-phenyl-3-(2-furyl)-2-propenal. The amount of potassiumis 50 g/kg dry matter and the amount of sodium is 3 g/kg dry matter.

For comparison, a liquid coffee concentrate is prepared in the samemanner as described above except that the heat treatment is omitted. Theresulting liquid coffee concentrate has a pH of 5.2. Within 6 weeks,this product drops below pH 5 (see FIG. 3 (▪)) When assessed by experttasters the product is unpleasantly sour.

Example 5 Extraction (Split Stream)

From a single batch of ground coffee, a coffee extract is obtained bysplit stream extraction as described in WO 2007/043873.

A 1^(st) primary extract (stream A in FIG. 6), the high aromatic coffeeextract, is left untreated. All of secondary extract (stream E) (about55 v/v %) is left untreated as well.

Processing

All of the 2^(nd) primary extract (stream C) (about 45/v %) is treatedby adjusting the pH to 6 by passing the extract over an anion column(Lewatit® XA 945).

The 2^(nd) primary extract is heated from ambient conditions to 180° C.in 6 minutes, and kept at that temperature for 2.5 consecutive minutes,followed by a cooling step of 2.5 minutes.

This process results in a hydrolysation of at least 176 mMoles acid/kgdry matter solids content in the final product

The heat treated 2^(nd) primary extract is mixed with the untreatedsecondary extract and concentrated.

The concentrated low aromatic coffee extract is mixed with the higharomatic coffee extract (1^(st) primary extract) (stream A).

The resulting pH of the liquid coffee concentrate is 5.27 and has a drymatter solids content of 28%.

No detectable off flavor is detected in the liquid coffee concentrateduring storage.

Example 6

A single batch of Arabic coffee is subjected to the extraction asdescribed in Example 2. The pH of the low aromatic coffee extractobtained therefrom with a dry matter solids content of approximately 6%is adjusted by addition of KOH to pH 6. The low aromatic coffee extractis heated from ambient conditions to 150° C. in approximately 3.5minutes and kept at that temperature for 10 consecutive minutes,followed by a cooling step of approximately 2.5 minutes. The heattreated low aromatic coffee extract is concentrated. The concentratedlow aromatic coffee extract is mixed with the high aromatic coffeeextract (1^(st) primary extract) (stream A).

The resulting pH of the liquid coffee concentrate is 5.4 and a drymatter solids content of 28%. This process results in a hydrolysation ofat least 220 mMoles acid/kg dry matter solids content in the finalproduct. No detectable off smell is detected in the liquid coffeeconcentrate but a metallic off taste was present due to the presence ofKOH.

The pH was followed in time as shown in FIG. 4 (▴). During 28 weeksshelf life the product does not drop in pH below 5. When assessed byexpert tasters, no unpleasant acidity can be detected in the product.

For comparison, a liquid coffee concentrate is prepared in the samemanner as described above except that the heat treatment is omitted. Theresulting liquid coffee concentrate has a pH of 5.2. Within 4 weeks,this product drops below pH 5 (see FIG. 4 (▪)). When assessed by experttasters the product is unpleasantly sour.

Comparative Example 7

A liquid coffee concentrate having approximate 30% w/w dry solids wasobtained by extraction a mixture of 50% Arabica and 50% Robusta coffeebeans and processed according to the steps described in US 2010/0316784.

The pH of the liquid coffee extract was adjusted to 5.7 by addition ofedible alkali, i.e. potassium hydroxide.

The resulting coffee concentrate was processed at 145° C. with a holdingtime of 90 seconds followed by rapid cooling to ambient condition.

The pH of the final product was approximately 5.2.

Only 100 mmoles acid/kg dry matter content in the final product werereleased. The pH dropped below 5.0 within 8 weeks.

When assessed by experts the product had a sour off taste.

What is claimed is:
 1. A liquid coffee concentrate with a pH of 4.8 to 6obtainable by a process comprising: subjecting roasted, ground coffee toone or more extraction steps with water resulting in a coffee extract;separating the coffee extract by fractionation during the extractionstep(s) resulting in a high aromatic coffee extract and a low aromaticcoffee extract, wherein the low aromatic coffee extract comprises asecond primary extract and a secondary extract; subjecting at least partof the second primary extract to a heat treatment of at least 120° C.for at most 30 minutes, wherein the part of the second primary extractto be treated comprises at least 25 v/v % of the low aromatic coffeeextract, resulting in a treated low aromatic coffee extract;concentrating at least the treated low aromatic coffee extract,resulting in a concentrated low aromatic coffee extract; and combiningat least the concentrated low aromatic coffee extract with the higharomatic coffee extract, thereby obtaining a liquid coffee concentrate,wherein the liquid coffee concentrate has a pH of 4.8 to
 6. 2. A liquidcoffee concentrate with a pH of 4.8 to 6 comprising 2 mg/kg dry mattersolids or more of 2-phenyl-3-(2-furyl)-2-propenal.
 3. A liquid coffeeconcentrate with a pH between 5 and 5.2 and a Quinic acid/Quinic acidlactone mol/mol ratio between 10 and
 100. 4. A liquid coffee concentrateaccording to claim 3, further comprising a potassium content of 55 g orless per kg dry matter and/or a sodium content of 4 g or less per kg drymatter.
 5. The liquid coffee concentrate of claim 3, wherein the Quinicacid/Quinic acid lactone mol/mol ratio is between 30 and 100.